CN106966388A - A kind of micro crystal graphite high-temperature fluorination method of purification - Google Patents
A kind of micro crystal graphite high-temperature fluorination method of purification Download PDFInfo
- Publication number
- CN106966388A CN106966388A CN201710293844.3A CN201710293844A CN106966388A CN 106966388 A CN106966388 A CN 106966388A CN 201710293844 A CN201710293844 A CN 201710293844A CN 106966388 A CN106966388 A CN 106966388A
- Authority
- CN
- China
- Prior art keywords
- micro crystal
- graphite
- crystal graphite
- purification
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of micro crystal graphite high-temperature fluorination method of purification, the natural micro crystal graphite that fixed carbon is 99.9% is taken, fluorization agent is added, delivers to and pyroreaction is carried out in serialization high temperature furnace, the natural micro crystal graphite that purity is more than 99.900% is obtained；The present invention uses fluorization agent and serialization high temperature furnace, the purification graphite of fixed carbon 99.9% to the graphite of fixed carbon 99.990 99.999%.
Description
Technical field
The present invention relates to the purification technique field of micro crystal graphite, more particularly to a kind of micro crystal graphite high-temperature fluorination purification side
Method.
Background technology
Micro crystal graphite has very important ground in some special industries or high-tech area as a kind of raw material of industry
Position, such as atomic energy industry, auto industry, space technology, biotechnology industry.Its is carbon containing for the micro crystal graphite that these industries are used
Amount must be more than 99.9% high-purity micro crystal graphite, and the phosphorus content of the natural micro crystal graphite after general ore dressing is up to
80% or so, by commonly reaching 99.5% after alkali fusion/pickling, the requirement using high-purity industry can not be much met, is this
Must be to the further purification of micro crystal graphite.
A kind of Patent No. 200910112366.7, entitled purification of microcrystalline graphite product makes new technology with purifying,
Comprise the following steps：Reach that mog is to add quick lime in the graphite raw ore that -200 mesh percent of pass are more than 90% in fine grinding
Stirred with water, make the pH of the graphite ore pulp containing quick lime>9, waterglass stirring, kerosene stirring are added, pine camphor is eventually adding
Bubble is scraped in oil stirring inflation, is carried out roughing, is collected graphite rougher concentration and mine tailing；The concentrate addition waterglass stirring of roughing acquisition,
Add kerosene stirring, addition terpenic oil to stir and inflate and scrape bubble, carry out primary cleaning, collect selected concentrate；The essence of primary cleaning
The stirring of ore deposit addition waterglass, the stirring of addition kerosene, addition terpenic oil are stirred and inflated and scrape bubble, and progress recleaning collects flotation
Graphite concentrate；Above-mentioned flotation graphite concentrate adds NaOH solution to carry out batch mixing, is calcined, is washed to neutrality, with hydrochloric acid acidleach, washes,
Dewatered drying, obtains graphite and fixes the high-carbon graphite product that carbon content reaches 98.74%；The purity of this method of purification does not reach
More than 99.90%, and operating method is excessively complicated, cost is high.
Patent No. CN90109672.5, a kind of entitled method for purifying high-carbon graphite, during application (patent right) is artificial
Xi'an optical precision optical machinery research institute of the academy of sciences of state, its technical scheme is：Using by hydrochloric acid, nitric acid (or sulfuric acid) and hydrofluoric acid group
Into mixed acid agent, under normal temperature (0 DEG C -65 DEG C), the raw material of low-carbon grade 2-4 days in wet-treating, remove impurity, produce and carry
Pure high-carbon graphite, the composition and its consumption of its mixed acid agent be according to the ore body composition of graphite raw material and the composition of ash content and its
Content difference and prepare, based on every hectogram graphite raw material, the excursion of each composition usage amount of mixed acid agent is：Concentrated hydrochloric acid
15-60ml, concentrated nitric acid (or concentrated sulfuric acid) 0-30ml, hydrofluoric acid (40%) 15-60ml above-mentioned various sour agent allow to change in proportion
Calculation uses diluted acid, can be separately added into, and can also be added with mixed acid, and water (or spent acid mother liquor) can then make as supplement
Obtain solution and flood graphite raw material, somewhat excessive to be advisable, daily stirring is for several times.This operating method is excessively complicated, and cost is high, and the time
It is long.
The content of the invention
There is provided that a kind of cost is low, steady quality it is an object of the invention to overcome above-mentioned weak point of the prior art
Micro crystal graphite high-temperature fluorination method of purification.
The present invention is realized in the following way：
A kind of micro crystal graphite high-temperature fluorination method of purification, it is characterised in that：It is 1 to take weight ratio：0.7-1.48 fixed carbon
For 99.9% natural micro crystal graphite and fluorization agent, deliver to and pyroreaction is carried out in serialization high temperature furnace, temperature is 2800-3000
DEG C, reaction time 10-60min obtains the natural micro crystal graphite that purity is more than 99.990%.
Preferably, the fluorization agent is one kind in poly- carbon tetrachloride, polytetrafluoroethylene (PTFE).
The beneficial effects of the present invention are：Using fluorization agent and serialization high temperature furnace, purification fixed carbon 99.9% graphite is extremely
Fixed carbon 99.990-99.999% graphite；Fluorization agent causes the impurity in graphite to remove more completely；Serialization high temperature furnace was operated
Journey can serialization, the error of reduction human factor.
Embodiment
The specific embodiment of the invention is now described in detail：
A kind of micro crystal graphite high-temperature fluorination method of purification, it is characterised in that：It is 1 to take weight ratio：0.75-1.45 fixed carbon
For 99.9% natural micro crystal graphite and fluorization agent, deliver to and pyroreaction is carried out in serialization high temperature furnace, temperature is 2800-3000
DEG C, reaction time 10-60min obtains the natural micro crystal graphite that purity is more than 99.990%.
Fluorization agent of the present invention is one kind in poly- carbon tetrachloride, polytetrafluoroethylene (PTFE).
Embodiment 1
The natural micro crystal graphite 30kg that fixed carbon 99.9% is is taken, poly- carbon tetrachloride 22.5-43.5kg is added, delivered to continuous
Change and pyroreaction is carried out in high temperature furnace, temperature is 2800-3000 DEG C, reaction time 30-60min, and being fixed carbon is
99.9992% high-purity natural micro crystal graphite.
Embodiment 2
It is natural micro crystal graphite 50kg to take fixed carbon 99.9%, adds polytetrafluoroethylene (PTFE) 37.5-72.5kg, delivers to serialization
Pyroreaction is carried out in high temperature furnace, temperature is 2800-3000 DEG C, reaction time 30-60min, and it is 99.9992% to be fixed carbon
High-purity natural micro crystal graphite.
Carbon content is fixed in the sample of two embodiments of the above, graphite products Quality Supervision and Inspection Center of warp let-off country
Detection, specific testing result is as follows：
Therefore, by present invention fluorization agent and serialization high temperature furnace the purification graphite of fixed carbon 99.9% can be realized to admittedly
Determine carbon 99.990-99.999% graphite.
Claims (2)
1. a kind of micro crystal graphite high-temperature fluorination method of purification, it is characterised in that：It is 1 to take weight ratio：0.7-1.48 fixed carbon is
99.9% natural micro crystal graphite and fluorization agent, delivers to and pyroreaction is carried out in serialization high temperature furnace, temperature is 2800-3000
DEG C, reaction time 10-60min obtains the natural micro crystal graphite that purity is more than 99.990%.
2. a kind of micro crystal graphite high-temperature fluorination method of purification according to claim 1, it is characterised in that：The fluorization agent is
One kind in poly- carbon tetrachloride, polytetrafluoroethylene (PTFE).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710293844.3A CN106966388A (en) | 2017-04-28 | 2017-04-28 | A kind of micro crystal graphite high-temperature fluorination method of purification |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710293844.3A CN106966388A (en) | 2017-04-28 | 2017-04-28 | A kind of micro crystal graphite high-temperature fluorination method of purification |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106966388A true CN106966388A (en) | 2017-07-21 |
Family
ID=59330393
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710293844.3A Pending CN106966388A (en) | 2017-04-28 | 2017-04-28 | A kind of micro crystal graphite high-temperature fluorination method of purification |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106966388A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112028069A (en) * | 2020-08-27 | 2020-12-04 | 中南钻石有限公司 | Preparation and method for purifying waste graphite in industrial diamond production |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102602908A (en) * | 2012-04-09 | 2012-07-25 | 上海尚饮思生化医药有限公司 | Purification method of battery-grade graphite fluoride |
| CN104211048A (en) * | 2013-06-05 | 2014-12-17 | 中国科学院上海有机化学研究所 | Preparation method of fluorinated graphene |
-
2017
- 2017-04-28 CN CN201710293844.3A patent/CN106966388A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102602908A (en) * | 2012-04-09 | 2012-07-25 | 上海尚饮思生化医药有限公司 | Purification method of battery-grade graphite fluoride |
| CN104211048A (en) * | 2013-06-05 | 2014-12-17 | 中国科学院上海有机化学研究所 | Preparation method of fluorinated graphene |
Non-Patent Citations (2)
| Title |
|---|
| 付甲尧: ""通气石墨化机理的探讨"", 《碳素》 * |
| 胡祥龙等: ""连续式高温反应石墨提纯装备与工艺"", 《新型炭材料》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112028069A (en) * | 2020-08-27 | 2020-12-04 | 中南钻石有限公司 | Preparation and method for purifying waste graphite in industrial diamond production |
| CN112028069B (en) * | 2020-08-27 | 2021-12-10 | 中南钻石有限公司 | Preparation and method for purifying waste graphite in industrial diamond production |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106966389A (en) | A kind of method of purification of micro crystal graphite | |
| CN106882805A (en) | A kind of micro crystal graphite purifies preparation technology | |
| CN105859167B (en) | A method of Gao Bai, high-pure anhydrous calcium sulfate are prepared by ardealite | |
| CN109290060A (en) | A kind of process for subsequent treatment and phosphate ore floatation method of phosphate ore flotation tailings | |
| CN103570043B (en) | Method for producing high-purity potassium chloride solution for preparation of potassium carbonate and co-producing low sodium salt | |
| CN109368612A (en) | Method for preparing battery-grade iron phosphate by using iron phosphate production wastewater and iron phosphate prepared by method | |
| CN113072046A (en) | Method for removing impurities and improving whiteness of phosphogypsum through flotation method | |
| CN107419335A (en) | The method that hydrochloric acid method Cycle-decomposition ardealite and phosphorus mine tailing prepare calcium sulfate crystal whiskers | |
| CN102701153B (en) | Treatment method for titanium dioxide process waste acid generated by molten salt chlorination process | |
| CN110408794A (en) | Asbestos deposit process for cleanly preparing | |
| CN106966388A (en) | A kind of micro crystal graphite high-temperature fluorination method of purification | |
| CN107056388A (en) | The preparation method of chemical polishing waste phosphoric acid processing method and fertilizer | |
| CN101597040B (en) | Method for producing food grade phosphoric acid with refined wet phosphoric acid and product thereof | |
| CN101575106A (en) | Coproduction technology of calcium sulphate crystal whiskers and magnesium hydrate crystal whiskers by plaster-ammonium rotation method | |
| WO2017173716A1 (en) | Method for joint production of phosphogypsum decomposition gas and wet-process phosphoric acid | |
| CN107459373A (en) | The method and system of potassium manganese mixed fertilizer are prepared based on graphene oxide generation spent acid | |
| CN101531384A (en) | Technique for preparing electronic grade magnesium hydrate and ammonium sulphate by cycle serum featuring in flue gas desulfurization by method of magnesium oxidization | |
| CN110732543B (en) | Method for jointly producing cement clinker and ammonia water by electrolyzing metal manganese waste residue and gypsum | |
| CN108455647A (en) | A kind of method of phosphoric acid by-product ardealite and fluosilicic acid production calcirm-fluoride by-product white carbon and ammonium sulfate | |
| CN107585789A (en) | A kind of method that high-purity molybdenum trioxide is prepared using hydrometallurgy molybdenum concntrate | |
| CN106350870A (en) | Disposal and utilization method for sulfuric acid waste liquid | |
| CA2566293C (en) | Tungstic acid powder consisting of spherical tungsten particles and method for producing same | |
| CN113292101B (en) | Preparation method and application of high-purity birnessite material | |
| CN101760630A (en) | Method for recovering copper from copper sulfate solution | |
| CN105330050A (en) | Integrated waste water treatment and resource recycle method of crystal processing |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170721 |
|
| RJ01 | Rejection of invention patent application after publication |